JPH04170403A - Aftertreatment of polybutadiene polymerization solution - Google Patents
Aftertreatment of polybutadiene polymerization solutionInfo
- Publication number
- JPH04170403A JPH04170403A JP29540090A JP29540090A JPH04170403A JP H04170403 A JPH04170403 A JP H04170403A JP 29540090 A JP29540090 A JP 29540090A JP 29540090 A JP29540090 A JP 29540090A JP H04170403 A JPH04170403 A JP H04170403A
- Authority
- JP
- Japan
- Prior art keywords
- polybutadiene
- phase
- polymerization solution
- solution
- deashing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000005062 Polybutadiene Substances 0.000 title claims abstract description 94
- 229920002857 polybutadiene Polymers 0.000 title claims abstract description 94
- 238000006116 polymerization reaction Methods 0.000 title claims description 60
- 239000002904 solvent Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000005191 phase separation Methods 0.000 claims abstract description 20
- 239000012071 phase Substances 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 23
- 239000008346 aqueous phase Substances 0.000 claims description 16
- 229920000642 polymer Polymers 0.000 claims 2
- 230000007423 decrease Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 43
- 239000003054 catalyst Substances 0.000 description 14
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 11
- 239000000203 mixture Substances 0.000 description 6
- IAQRGUVFOMOMEM-ARJAWSKDSA-N cis-but-2-ene Chemical compound C\C=C/C IAQRGUVFOMOMEM-ARJAWSKDSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000012805 post-processing Methods 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- QNRMTGGDHLBXQZ-UHFFFAOYSA-N buta-1,2-diene Chemical compound CC=C=C QNRMTGGDHLBXQZ-UHFFFAOYSA-N 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005261 decarburization Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 230000011514 reflex Effects 0.000 description 1
- IAQRGUVFOMOMEM-ONEGZZNKSA-N trans-but-2-ene Chemical compound C\C=C\C IAQRGUVFOMOMEM-ONEGZZNKSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、溶液重合法で得られたポリブタジェン重合溶
液の後処理方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for post-treatment of a polybutadiene polymerization solution obtained by a solution polymerization method.
本発明の後処理方法は、チーグラー・ナツタ系触媒や有
機Ｌｉ系触媒を触媒として１． ３−ブタジェンを溶液
重合して得られたポリブタジェン重合溶液の脱灰処理及
び濃縮処理に、特に好ましく用いることができる。The post-treatment method of the present invention includes 1. using a Ziegler-Natsuta catalyst or an organic Li catalyst as a catalyst. It can be particularly preferably used for deashing and concentrating a polybutadiene polymerization solution obtained by solution polymerizing 3-butadiene.
ポリブタジェンは、通常、１．３−ブタジェンの溶液重
合により製造されている。そして、触媒にはチーグラー
・ナツタ系触媒や有機Ｌｉ系触媒か用いられている。Polybutadiene is usually produced by solution polymerization of 1,3-butadiene. As a catalyst, a Ziegler-Natsuta catalyst or an organic Li-based catalyst is used.
そして、重合終了後、ポリブタジェン重合溶液を脱灰し
て触媒を除去してから、濃縮及び脱揮によってポリブタ
ジェンを回収する。After the polymerization is completed, the polybutadiene polymerization solution is deashed to remove the catalyst, and then the polybutadiene is recovered by concentration and devolatilization.
ところて、これらのチーグラー・ナツタ系触媒や有機Ｌ
ｉ系触媒は水により容易に分解し、水溶性の化合物にな
る。そこて、ポリブタジェン重合溶液に水を加えて混合
、水洗し、その後水相を除去することにより、脱灰を行
っている。By the way, these Ziegler-Natsuta catalysts and organic L
The i-type catalyst is easily decomposed by water and becomes a water-soluble compound. Therefore, deashing is performed by adding water to the polybutadiene polymerization solution, mixing it, washing with water, and then removing the aqueous phase.
従来は、ポリブタジェン重合溶液の脱灰においては、水
を加え静置するという方法が行われていた。Conventionally, the method of deashing a polybutadiene polymerization solution was to add water and leave it to stand still.
しかし、水を加えたポリブタジェン重合溶液を単に静置
しただけでは水相と重合溶媒相との分離か悪く、分離に
時間かかかる上、ポリブタジェン重合溶液から充分に水
か除去されないという問題かあった。However, simply leaving the polybutadiene polymerization solution to which water has been added results in poor separation of the aqueous phase and polymerization solvent phase, which takes time, and there are problems in that water is not sufficiently removed from the polybutadiene polymerization solution. .
本発明は、上記の問題を解決した後処理方法を提供する
ことを目的とする。An object of the present invention is to provide a post-processing method that solves the above problems.
即ち、水を加えたポリブタジェン重合溶液から完全に水
相を除去てきる後処理方法を提供することを目的とする
。That is, the object of the present invention is to provide a post-treatment method that can completely remove the aqueous phase from a polybutadiene polymerization solution to which water has been added.
本発明は、
（ａ）ポリブタジェン重合溶液に水を加え、（ｂ）この
ポリブタジェン重合溶液を脱灰層の水相中に噴射し、
（ｃ）次いで水相と重合溶媒相に分離して脱灰する、ポ
リブタジェン重合溶液の後処理方法、に関する。The present invention comprises: (a) adding water to a polybutadiene polymerization solution; (b) injecting this polybutadiene polymerization solution into an aqueous phase of a deashing layer; (c) then separating into an aqueous phase and a polymerization solvent phase for deashing. The present invention relates to a method for post-treatment of a polybutadiene polymerization solution.
更に、上記の方法によって脱灰したポリブタジェン重合
溶液を、
（ｄ）相分離の起こる温度下で、相分離槽のポリブタジ
ェン希薄相へ導入し、ポリブタジェン希薄相（上層）と
ポリブタジェン濃厚相（下層）に分離して、
ポリブタジェン濃厚溶液を得る、
方法も含む。Furthermore, the polybutadiene polymerization solution deashed by the above method is introduced into the polybutadiene dilute phase of the phase separation tank (d) at a temperature at which phase separation occurs, and the polybutadiene dilute phase (upper layer) and the polybutadiene concentrated phase (lower layer) are separated. Also included is a method of separating to obtain a concentrated polybutadiene solution.
本発明の後処理方法のプロセスフローの一例を第１図の
プロセス図に示す。An example of the process flow of the post-processing method of the present invention is shown in the process diagram of FIG.
以下、このプロセス図に従って、本発明を説明する。Hereinafter, the present invention will be explained according to this process diagram.
先ず、触媒を分解するためポリブタジェン重合溶液に水
を加え混合する。混合はミキサーや攪拌機等により行う
ことがてきる。ポリブタジェン重合溶液に水を加えるこ
とにより、触媒か分解し、水相に移行する。ポリブタジ
ェン重合溶液に加える水の量は、このポリブタジェン重
合溶液に対してｌＯ〜４０容量％の範囲が好ましい。ま
た、このときのポリブタジェン重合溶液の温度は、臨界
温度未満の温度即ち相分離の起こらない範囲の温度か好
ましい。この範囲の温度であれば、触媒か水と充分接触
し完全に分解するからである。First, water is added to the polybutadiene polymerization solution and mixed to decompose the catalyst. Mixing can be performed using a mixer, a stirrer, or the like. By adding water to the polybutadiene polymerization solution, the catalyst is decomposed and transferred to the aqueous phase. The amount of water added to the polybutadiene polymerization solution is preferably in the range of 10 to 40% by volume based on the polybutadiene polymerization solution. Further, the temperature of the polybutadiene polymerization solution at this time is preferably a temperature below the critical temperature, that is, a temperature within a range where phase separation does not occur. This is because if the temperature is within this range, the catalyst will come into sufficient contact with water and will be completely decomposed.
続いて、このポリブタジェン重合溶液を脱灰槽の水相中
に噴射して、重合溶媒相と水相とに分離する。このとき
の重合溶液の温度は、臨界温度以上の温度、即ち相分離
が起こる範囲の温度であることか好ましい。臨界温度以
上の温度では水の分離か容易に起こるからである。但し
、余りポリブタジェン重合溶液の温度か高いと、ポリブ
タジェン濃厚相の粘度か高くなり過ぎ脱灰効率か低下し
好ましくない。従って、最も好ましい温度範囲は、臨界
温度乃至臨界温度より２０°Ｃ高い範囲である。Subsequently, this polybutadiene polymerization solution is injected into the aqueous phase of the deashing tank to separate it into a polymerization solvent phase and an aqueous phase. The temperature of the polymerization solution at this time is preferably a temperature equal to or higher than the critical temperature, that is, a temperature within a range where phase separation occurs. This is because water separation easily occurs at temperatures above the critical temperature. However, if the temperature of the polybutadiene polymerization solution is too high, the viscosity of the polybutadiene concentrated phase becomes too high and the deashing efficiency decreases, which is not preferable. Therefore, the most preferred temperature range is between the critical temperature and 20°C above the critical temperature.
ここで、臨界温度とは、ポリブタジェン重合溶液の相分
離か起こる温度をいい、圧力、溶媒の種類や組成、ポリ
ブタジェンの濃度や分子量によって決まる温度である。Here, the critical temperature refers to the temperature at which phase separation of the polybutadiene polymerization solution occurs, and is determined by the pressure, the type and composition of the solvent, and the concentration and molecular weight of the polybutadiene.
−例として、シス−２−ブテンを主成分とするＣ４溶媒
を溶媒とするポリブタジェンの溶液について、ポリブタ
ジェン濃度と臨界温度との関係を示す（第２図）。- As an example, the relationship between polybutadiene concentration and critical temperature is shown for a solution of polybutadiene in a C4 solvent containing cis-2-butene as a main component (Figure 2).
脱灰槽て水相を分離し触媒を除去したポリブタジェン重
合溶液を一次濃縮したのち脱揮押出機等で溶媒を除去す
ることにより、ポリブタジェンを回収することかできる
。The polybutadiene can be recovered by first concentrating the polybutadiene polymerization solution from which the aqueous phase is separated in a deashing tank and the catalyst is removed, and then the solvent is removed using a devolatilizing extruder or the like.
一次濃縮には、相分離を利用することができる。Phase separation can be used for primary concentration.
具体的には、臨界温度以上の温度でポリブタジェン重合
溶液を相分離槽のポリブタジェン希薄相へ導入し、ポリ
ブタジェン希薄相（上層）と、ポリブタジェン濃厚相（
下層）に分離する等の方法か可能である。ここで、ポリ
ブタジェン希薄相は低分子量のポリブタジェン溶液であ
る。一方、ポリブタジェン濃厚相はポリブタジェン濃度
か２０〜４０重量％と高いポリブタジェン溶液である。Specifically, a polybutadiene polymerization solution is introduced into a polybutadiene dilute phase of a phase separation tank at a temperature higher than the critical temperature, and a polybutadiene dilute phase (upper layer) and a polybutadiene concentrated phase (
It is possible to separate it into a lower layer). Here, the polybutadiene dilute phase is a low molecular weight polybutadiene solution. On the other hand, the polybutadiene concentrated phase is a polybutadiene solution with a high polybutadiene concentration of 20 to 40% by weight.
ポリブタジェン希薄層は系外に捨ててもよいが、必要に
応じて濃縮により重合溶媒と未反応１，３−ポリブタジ
ェンを除去し、ポリブタジェン濃厚相に戻してもよい。The polybutadiene dilute layer may be discarded outside the system, but if necessary, the polymerization solvent and unreacted 1,3-polybutadiene may be removed by concentration and returned to the polybutadiene rich phase.
ポリブタジェン重合溶液の一次濃縮は、この他、フラッ
シュ蒸発法等、公知の方法により行ってもよい。In addition to this, the primary concentration of the polybutadiene polymerization solution may be performed by a known method such as a flash evaporation method.
本発明の後処理方法を適用できるポリブタジェン重合溶
液は、ベンゼンやトルエン、キシレン等の芳香族系炭化
水素溶媒や、ブタン、ヘプタンやｎ−ヘキサン等の脂肪
族系炭化水素溶媒、もしくはブテン等のすレフイン系炭
化水素溶媒、又はこれらの溶媒の混合物等を重合溶媒と
するものである。特に、シス−２−ブテンを主成分とす
る炭化水素混合物であるＣ４留分を重合溶媒とするポリ
ブタジェン重合溶液に対して、本発明の方法は好適であ
る。The polybutadiene polymerization solution to which the post-treatment method of the present invention can be applied is an aromatic hydrocarbon solvent such as benzene, toluene, or xylene, an aliphatic hydrocarbon solvent such as butane, heptane, or n-hexane, or a solvent such as butene. The polymerization solvent is a reflex hydrocarbon solvent or a mixture of these solvents. In particular, the method of the present invention is suitable for a polybutadiene polymerization solution using a C4 fraction, which is a hydrocarbon mixture containing cis-2-butene as a main component, as a polymerization solvent.
以下に、本発明の実施例を示す。 Examples of the present invention are shown below.
実施例１
・ １．３−ブタジェン３０重量％、シス−２−ブテ
ン５６重量％、トランス−２−ブテン１３重量％、残部
ｎ−ブタン、プロパン、エタン等、なる組成の１，３−
ブタジェン溶液に、コバルトオクトエート−水−ジエチ
ルアルミニウムモノクロライド系触媒、及び１，２−ブ
タジェンを添加して１．３−ブタジェンの重合を行った
。重合後、２゜６−ｔ−ブチルフェノール及び水を添加
して重合を停止し、ポリブタジェン重合溶液を得た。こ
のポリブタジェン重合溶液のポリブタジェン濃度は１６
重量％であった。そして、ポリブタジェンのムーニー粘
度は４３、シス−１，４結合の含有率は９８．５％であ
った。このポリブタジェン重合溶媒の臨界温度は４８°
Ｃであった。Example 1 - 1,3-butadiene having a composition of 30% by weight, 56% by weight of cis-2-butene, 13% by weight of trans-2-butene, and the balance being n-butane, propane, ethane, etc.
A cobalt octoate-water-diethylaluminum monochloride catalyst and 1,2-butadiene were added to the butadiene solution to polymerize 1,3-butadiene. After the polymerization, 2°6-t-butylphenol and water were added to stop the polymerization, and a polybutadiene polymerization solution was obtained. The polybutadiene concentration of this polybutadiene polymerization solution is 16
% by weight. The Mooney viscosity of polybutadiene was 43, and the content of cis-1,4 bonds was 98.5%. The critical temperature of this polybutadiene polymerization solvent is 48°
It was C.
このポリブタジェン重合溶液ＩＯＡに対して、水を３１
の割合で混入し、ミキサーで混合した。Add 31% water to this polybutadiene polymerization solution IOA.
and mixed with a mixer.
このときの温度は相分離の起こらない４０°Ｃとした。The temperature at this time was 40°C at which phase separation did not occur.
ついで、このポリブタジェン重合溶液を熱交換器で６０
°Ｃに加温し、内容量２０１、内部温度６０°Ｃの脱灰
槽の水相中に噴射した。噴射量は毎時１３１とした。ポ
リブタジェン重合溶液は上層の重合溶媒相と下層の水相
に分離した。そして、重合溶媒相はポリブタジェン希薄
相とポリブタジェン濃厚相の二層に分離していた。Next, this polybutadiene polymerization solution was heated at 60°C in a heat exchanger.
The mixture was heated to 60°C and injected into the aqueous phase of a deashing tank with an internal capacity of 201°C and an internal temperature of 60°C. The injection amount was 131 per hour. The polybutadiene polymerization solution was separated into an upper polymerization solvent phase and a lower aqueous phase. The polymerization solvent phase was separated into two layers: a polybutadiene dilute phase and a polybutadiene concentrated phase.
この重合溶媒層を脱灰槽より抜き出し、内容量１０Ｉ！
の相分離槽のポリブタジェン希薄相に供給した。相分離
槽内は温度７０°Ｃ１圧力９ｋｇｆ／ｃｎｆＡに保持し
た。This polymerization solvent layer was extracted from the deashing tank, and the content was 10 I!
was fed to the polybutadiene dilute phase of the phase separation tank. The inside of the phase separation tank was maintained at a temperature of 70° C., a pressure of 9 kgf/cnfA.
相分離槽でポリブタジェン希薄相とポリブタジェン濃厚
相に５８：４２の割合で分離した。ポリブタジェン希薄
相のポリブタジェン濃度は１．５重量％、ポリブタジェ
ン濃厚相のポリブタジェン濃度は３３重量％であった。The mixture was separated into a polybutadiene dilute phase and a polybutadiene rich phase in a ratio of 58:42 in a phase separation tank. The polybutadiene concentration in the polybutadiene dilute phase was 1.5% by weight, and the polybutadiene concentration in the polybutadiene rich phase was 33% by weight.
相分離槽の上層からポリブタジェン希薄相を毎時５．８
Ｉ！の割合で抜取り、これを熱交換器に通し、蒸発槽
で未反応１，３−ブタジェン及び溶媒を蒸発、除去して
、ポリブタジェン濃度を３３％とした。ついで、これを
毎時０．２１、ポリブタジェン濃厚相を毎時４．２１の
割合で混合し、濃縮ポリブタジェン溶液を得た。Polybutadiene dilute phase is extracted from the upper layer of the phase separation tank at a rate of 5.8% per hour.
I! This was passed through a heat exchanger, and unreacted 1,3-butadiene and the solvent were evaporated and removed in an evaporation tank to give a polybutadiene concentration of 33%. This was then mixed at a rate of 0.21/hour and the polybutadiene concentrated phase at a rate of 4.21/hour to obtain a concentrated polybutadiene solution.
脱揮押出機で、この濃縮ポリブタジェン溶液から重合溶
媒及び未反応１．３−ブタジェンを除去してポリブタジ
ェンを得た。Polybutadiene was obtained by removing the polymerization solvent and unreacted 1,3-butadiene from this concentrated polybutadiene solution using a devolatilizing extruder.
このポリブタジェンの灰分は、０．０３重量％であった
。The ash content of this polybutadiene was 0.03% by weight.
本発明の後処理方法においては、水を加えて重合触媒を
分解したポリブタジェン重合溶液を、相分離の起こる範
囲の温度で、脱灰槽の水相に、ノズル等を通して噴射す
る。In the post-treatment method of the present invention, a polybutadiene polymerization solution in which water has been added to decompose the polymerization catalyst is injected into the aqueous phase of the deashing tank through a nozzle or the like at a temperature within a range where phase separation occurs.
これにより、水相と重合溶媒相とか短時間で良好に分離
する。As a result, the aqueous phase and polymerization solvent phase can be separated well in a short time.
従って、脱灰の所要時間か大幅に短縮できる効果かある
。Therefore, the time required for decalcification can be significantly shortened.
更に、脱炭後の一次濃縮に相分離を利用することにより
、ポリブタジェン重合溶液の溶液粘度か高い状態におい
ても効果的に濃縮てきる。Furthermore, by utilizing phase separation for the primary concentration after decarburization, it is possible to effectively concentrate the polybutadiene polymerization solution even when the solution viscosity is high.
第１図は、本発明の後処理方法の一例を示す工程図であ
る。
第２図は、シス−２−ブテンを主成分とするＣ４溶媒を
溶媒とするポリブタジェンの溶液について、ポリブタジ
ェン濃度と臨界温度との関係を示す相図である。FIG. 1 is a process diagram showing an example of the post-processing method of the present invention. FIG. 2 is a phase diagram showing the relationship between polybutadiene concentration and critical temperature for a polybutadiene solution using a C4 solvent containing cis-2-butene as a main component.
Claims (4)
噴射し、 （ｃ）次いでこのポリブタジエン重合溶液を水相と重合
溶媒相に分離し、水相を除去して脱灰する、ポリブタジ
エン重合溶液の後処理方法、(1) (a) Add water to the polybutadiene polymerization solution, (b) Inject this polybutadiene polymerization solution into the water phase of the deashing layer, (c) Then separate this polybutadiene polymerization solution into the water phase and the polymerization solvent phase. A method for post-treatment of a polybutadiene polymer solution, which comprises removing the aqueous phase and deashing the polybutadiene polymer solution;
噴射し、 （ｃ）次いでこのポリブタジエン重合溶液を水相と重合
溶媒相に分離して、水相を除去して脱灰し、 （ｄ）このポリブタジエン重合溶液を、相分離が起こる
温度下で、相分離槽のポリブタジエン希薄相へ導入し、
ポリブタジエン希薄相（上層）とポリブタジエン濃厚相
（下層）に分離する、ポリブタジエン重合溶液の後処理
方法。(2) (a) Adding water to the polybutadiene polymerization solution, (b) Injecting this polybutadiene polymerization solution into the aqueous phase of the deashing layer, (c) Then separating this polybutadiene polymerization solution into an aqueous phase and a polymerization solvent phase. (d) introducing the polybutadiene polymerization solution into the polybutadiene dilute phase of a phase separation tank at a temperature at which phase separation occurs;
A post-treatment method for a polybutadiene polymerization solution that separates the polybutadiene dilute phase (upper layer) and polybutadiene concentrated phase (lower layer).
温度で行う、特許請求の範囲第１項又は第２項に記載の
後処理方法。(3) The post-treatment method according to claim 1 or 2, wherein the step (a) is carried out at a temperature within a range where phase separation does not occur.
範囲の温度で行う、特許請求の範囲第１項乃至第３項に
記載の後処理方法。(4) The post-treatment method according to any one of claims 1 to 3, wherein the step (b) is carried out at a temperature within a range where phase separation of the polymerization solution occurs.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2295400A JP2890803B2 (en) | 1990-11-02 | 1990-11-02 | Post-treatment method for polybutadiene polymerization solution |
| EP91118588A EP0484826A1 (en) | 1990-11-02 | 1991-10-31 | Method of post-treating polybutadiene solution |
| CA 2054790 CA2054790A1 (en) | 1990-11-02 | 1991-11-01 | Method of post-treating polybutadiene solution |
| TW80108627A TW205556B (en) | 1990-11-02 | 1991-11-02 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2295400A JP2890803B2 (en) | 1990-11-02 | 1990-11-02 | Post-treatment method for polybutadiene polymerization solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04170403A true JPH04170403A (en) | 1992-06-18 |
| JP2890803B2 JP2890803B2 (en) | 1999-05-17 |
Family
ID=17820121
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2295400A Expired - Fee Related JP2890803B2 (en) | 1990-11-02 | 1990-11-02 | Post-treatment method for polybutadiene polymerization solution |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2890803B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015105279A (en) * | 2013-11-28 | 2015-06-08 | 株式会社クラレ | Curable resin composition |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5222395A (en) * | 1975-08-13 | 1977-02-19 | Nippon Kayaku Kk | Novel hardening liquid used for dental cement |
-
1990
- 1990-11-02 JP JP2295400A patent/JP2890803B2/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5222395A (en) * | 1975-08-13 | 1977-02-19 | Nippon Kayaku Kk | Novel hardening liquid used for dental cement |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015105279A (en) * | 2013-11-28 | 2015-06-08 | 株式会社クラレ | Curable resin composition |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2890803B2 (en) | 1999-05-17 |
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